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| Simultaneous Determination of 26 Quinolones in Honey by UPLC－MS/MS with On-line Solid-phase Extraction and Isotope Dilution |
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| DOI： |
| KeyWord:on-line solid-phase extraction ultra performance liquid chromatography－tandem mass spectrometry quinolones honey |
| Author | Institution |
| ZHANG Ju-zhou，LI Jing |
1. Anhui Provincial Institute for Food and Drug Control，Hefei ，China; 2. China National Center for Quality Supervision and Test of Agricultural－Avocation Processed Food，Hefei ，China |
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| Abstract: |
| An on-line solid-phase extraction/ultra performance liquid chromatography－tandem mass spectrometric（SPE/UPLC－MS/MS） method was developed for the determination of twenty-six quinolone residues in honey．Firstly，the samples were extracted with 1% formic acid solution－methanol（10∶90），then rapidly purified by solid-phase extraction using an Oasis PRiME HLB cartridge．During the process，the key factors，such as the extraction solvent and purification method were optimized individually．The analytes were separated on an Agilent Eclipse Plus RRHD C18 column（2.1 mm × 50 mm，1.8 μm） by gradient elution，using water containing 0.1% formic acid and acetonitrile as the mobile phases．The target compounds were analyzed with electrospray ion source in positive ion mode under dynamic multi-reaction monitoring（dMRM） mode，and quantified by internal standard method．Results showed that there were good linear relationships for 26 quinolones in their respective concentration ranges with correlation coefficients（r2） more than 0.997．The limits of quantitation（LOQ） were in the range of 0.5－2.0 μg/kg．The average recoveries for 26 quinolones at low，medium and high spiked levels ranged from 79.5% to 110%，with relative standard deviations（RSD，n = 6） of 2.0%－12%．The developed method was rapid and accurate，which was suitable for the simultaneous screening and quantitative determination of 26 quinolones in honey． |
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